WO2019049632A1 - 半導体装置の製造方法、および、半導体装置 - Google Patents

半導体装置の製造方法、および、半導体装置 Download PDF

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WO2019049632A1
WO2019049632A1 PCT/JP2018/030517 JP2018030517W WO2019049632A1 WO 2019049632 A1 WO2019049632 A1 WO 2019049632A1 JP 2018030517 W JP2018030517 W JP 2018030517W WO 2019049632 A1 WO2019049632 A1 WO 2019049632A1
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semiconductor
forming
insulator layer
semiconductor layer
layer
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PCT/JP2018/030517
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English (en)
French (fr)
Japanese (ja)
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忠正 小林
秀昭 座間
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株式会社アルバック
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Priority to JP2019540859A priority Critical patent/JP6763093B2/ja
Priority to US16/346,243 priority patent/US11411120B2/en
Priority to KR1020197013700A priority patent/KR102229705B1/ko
Priority to CN201880004039.7A priority patent/CN109891559B/zh
Publication of WO2019049632A1 publication Critical patent/WO2019049632A1/ja

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    • H—ELECTRICITY
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    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
    • H01L29/76—Unipolar devices, e.g. field effect transistors
    • H01L29/772—Field effect transistors
    • H01L29/78—Field effect transistors with field effect produced by an insulated gate
    • H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
    • H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/42—Silicides
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
    • H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
    • H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
    • H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/36—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the concentration or distribution of impurities in the bulk material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/66007—Multistep manufacturing processes
    • H01L29/66075—Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials
    • H01L29/66227—Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials the devices being controllable only by the electric current supplied or the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched, e.g. three-terminal devices
    • H01L29/66409—Unipolar field-effect transistors
    • H01L29/66477—Unipolar field-effect transistors with an insulated gate, i.e. MISFET
    • H01L29/66742—Thin film unipolar transistors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
    • H01L29/76—Unipolar devices, e.g. field effect transistors
    • H01L29/772—Field effect transistors
    • H01L29/78—Field effect transistors with field effect produced by an insulated gate
    • H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
    • H01L29/78606—Thin film transistors, i.e. transistors with a channel being at least partly a thin film with supplementary region or layer in the thin film or in the insulated bulk substrate supporting it for controlling or increasing the safety of the device
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/01—Chemical elements
    • H01L2924/0103—Zinc [Zn]
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/01—Chemical elements
    • H01L2924/01049—Indium [In]

Definitions

  • the present invention relates to a method of manufacturing a semiconductor device including a semiconductor layer mainly containing an oxide semiconductor, and a semiconductor device.
  • a configuration including a semiconductor layer formed on a gate insulator layer covering a gate electrode and an insulator layer formed on a semiconductor layer is known. There is. A metal layer is formed on the insulator layer and the portion of the semiconductor layer not covered by the insulator layer. When forming a source electrode and a drain electrode from this metal layer, the insulator layer functions as an etching stopper layer.
  • Such an insulator layer is, for example, a silicon oxide (SiO 2 ) layer (see, for example, Patent Document 1).
  • a silicon oxide layer may be formed using plasma CVD method.
  • silane (SiH 4 ) or tetraethoxysilane (TEOS) is often used as a raw material for the silicon oxide layer. Since these materials contain hydrogen, the silicon oxide layer formed over the semiconductor layer also contains hydrogen. Hydrogen in the silicon oxide layer diffuses toward the semiconductor layer at the interface between the silicon oxide layer and the semiconductor layer to reduce oxygen in the semiconductor layer by reducing the semiconductor layer. Such oxygen deficiency in the semiconductor layer destabilizes the characteristics of the thin film transistor including the semiconductor layer and hence the characteristics of the semiconductor device provided with the thin film transistor. Therefore, a method for manufacturing a semiconductor device with more stable characteristics is required.
  • An object of the present invention is to provide a method of manufacturing a semiconductor device capable of stabilizing the characteristics of the semiconductor device, and a semiconductor device.
  • One aspect is a method of manufacturing a semiconductor device. This method includes forming a semiconductor layer including a surface and containing an oxide semiconductor as a main component, and containing silicon oxide as the main component and having a hydrogen atom concentration of 1 ⁇ 10 6 on the surface of the semiconductor layer. Forming an insulator layer having 21 pieces / cm 3 or less.
  • the semiconductor device is a semiconductor layer which includes a surface and is mainly composed of an oxide semiconductor, and an insulator layer located on the surface of the semiconductor layer, which is mainly composed of silicon oxide and has a hydrogen atom concentration of 10 And the insulator layer having 21 pieces / cm 3 or less.
  • the inventors of the present invention have found the following, while earnestly studying a semiconductor device including a semiconductor layer and an insulator layer located on the semiconductor layer. That is, in the insulator layer containing silicon oxide as a main component, when the concentration of hydrogen atoms is 1 ⁇ 10 21 atoms / cm 3 or less, the concentration of hydrogen atoms is greater than 1 ⁇ 10 21 atoms / cm 3 On the other hand, it has been found that oxygen deficiency generated in the semiconductor layer is significantly suppressed, whereby the characteristics of the semiconductor device are stabilized. In this respect, according to the above configuration, the insulator layer having a hydrogen atom concentration of 1 ⁇ 10 21 atoms / cm 3 or less can be formed, so that the characteristics of the semiconductor device can be stabilized.
  • forming the semiconductor layer may include forming at least one semiconductor layer whose main component is an oxide semiconductor.
  • the main component of the at least one semiconductor layer is an oxide semiconductor containing indium (In) and oxygen (O), and an oxide semiconductor containing zinc (Zn) and oxygen (O) It may be any one.
  • the main component of the at least one semiconductor layer may be any one selected from the group consisting of InGaZnO, GaZnO, InZnO, InTiZnO, InAlZnO, ZnAlO, ZnO, ZnAlO, and ZnCuO.
  • the semiconductor layer can include at least one semiconductor layer whose main component is an oxide semiconductor.
  • the main component of the at least one semiconductor layer is an oxide semiconductor containing indium (In) and oxygen (O), and an oxide semiconductor containing zinc (Zn) and oxygen (O) It may be any one.
  • the main component of the at least one semiconductor layer may be any one selected from the group consisting of InGaZnO, GaZnO, InZnO, InTiZnO, InAlZnO, ZnAlO, ZnO, ZnAlO, and ZnCuO.
  • forming the insulator layer may include forming the insulator layer by a plasma CVD method using a source gas and an oxygen-containing gas.
  • the source gas is preferably a gas containing silicon and an isocyanate group and containing no hydrogen.
  • forming the insulator layer may be performed by using, as the source gas, Si (NCO) 4 , Si (NCO) 3 Cl, Si (NCO) 2 Cl 2 , and Si (NCO). It may include using any one selected from the group consisting of Cl 3 .
  • forming the insulator layer is selected from the group consisting of O 2 , O 3 , N 2 O, CO, and CO 2 as the oxygen-containing gas. It may involve using one or more.
  • forming the insulator layer includes supplying the source gas and the oxygen-containing gas to a film forming space for forming the insulator layer to generate a mixed gas. And supplying electric power to an electrode located in the film formation space to generate plasma from the mixed gas.
  • the active species generated from the source gas is oxidized by the active species generated from the oxygen gas.
  • forming the insulator layer may use tetraisocyanatesilane gas as a source gas, and the ratio of the power supplied to the electrode to the flow rate of the tetraisocyanatesilane gas may be 17 W / sccm. It is preferable to include setting above.
  • the present inventors have found the following things while earnestly studying a method of manufacturing a semiconductor device. That is, when the insulator layer is formed by plasma CVD using tetraisocyanate silane gas and oxygen gas, the ratio of the power supplied to the electrode to the flow rate of tetraisocyanate silane gas is 17 W / sccm or more. It has been found that the certainty that the concentration of hydrogen atoms contained in the insulator layer is 1 ⁇ 10 21 atoms / cm 3 or less is enhanced. In this respect, according to the above configuration, the reliability of forming the insulator layer having a concentration of hydrogen atoms of 1 ⁇ 10 21 atoms / cm 3 or less is enhanced.
  • the block diagram which shows schematic structure of the sputter apparatus which is an example of the apparatus used for formation of a semiconductor layer in one Embodiment in the manufacturing method of a semiconductor device.
  • the block diagram which shows schematic structure of the plasma CVD apparatus which is an example of the apparatus used for formation of an insulator layer.
  • Sectional drawing which shows the cross-section of the semiconductor device in one Embodiment of a thin-film transistor.
  • concentration of the nitrogen atom in an insulator layer The graph which shows the relationship between high frequency electric power and the refractive index in an insulator layer.
  • 7 is a graph showing the relationship between the concentration of hydrogen atoms and the carrier concentration in the insulator layer.
  • 6 is a graph showing voltage-current characteristics of the thin film transistor of Example 1.
  • 6 is a graph showing voltage-current characteristics of the thin film transistor of Comparative Example 1;
  • a method of manufacturing a semiconductor device and an embodiment of the semiconductor device will be described with reference to FIGS. 1 to 12.
  • a method of manufacturing a semiconductor device, a configuration of a thin film transistor, a test example, and an example will be described in order.
  • a method of manufacturing a semiconductor device includes forming a semiconductor layer and forming an insulator layer.
  • Forming a semiconductor layer includes forming a semiconductor layer that includes a surface and is mainly composed of an oxide semiconductor.
  • an insulator layer which is mainly composed of silicon oxide (SiO 2 ) and has a hydrogen atom concentration of 1 ⁇ 10 21 atoms / cm 3 or less is formed on the surface of the semiconductor layer. To do.
  • the characteristics of the semiconductor device can be stabilized since the insulator layer having a concentration of hydrogen atoms of 1 ⁇ 10 21 atoms / cm 3 or less is formed.
  • a sputtering apparatus which is an example of an apparatus used for forming a semiconductor layer
  • the example of an apparatus used for forming an insulator layer will be described with reference to FIG.
  • the configuration of the plasma CVD apparatus will be described. Note that a semiconductor layer whose main component is the above-described oxide semiconductor may be formed using an apparatus other than a sputtering apparatus. Alternatively, the insulator layer may be formed using an apparatus other than a plasma CVD apparatus.
  • the sputtering apparatus 10 is equipped with the vacuum chamber 11 which divides the film-forming space for forming a semiconductor layer, and the film-forming object S in which a semiconductor layer is formed into a film inside the vacuum chamber 11
  • a support 12 supporting the is located.
  • the support unit 12 is, for example, a stage that supports the film formation target S.
  • a cathode 13 for forming a semiconductor layer is located at a position facing the support portion 12 in the vacuum chamber 11.
  • the cathode 13 includes a target 13a and a backing plate 13b.
  • the main component of the target 13a is an oxide semiconductor, and the oxide semiconductor is any one selected from the group consisting of InGaZnO (IGZO), GaZnO, InZnO, InTiZnO, InTiZnO, InAlZnO, ZnTiO, ZnO, ZnAlO, and ZnCuO.
  • IGZO InGaZnO
  • GaZnO GaZnO
  • InZnO InZnO
  • InTiZnO InTiZnO
  • InAlZnO InAlZnO
  • ZnTiO ZnTiO
  • ZnO, ZnAlO, and ZnCuO One is preferred. 90% by mass or more of the target 13a is an oxide semiconductor.
  • forming a semiconductor layer may be performed by forming one semiconductor layer containing any one selected from the group of oxide semiconductors described above as a main component, or forming two or more semiconductor layers.
  • forming a semiconductor layer can include forming at least one semiconductor layer containing an oxide semiconductor as a main component.
  • each semiconductor layer mainly includes any one selected from the group consisting of InGaZnO, GaZnO, InZnO, InTiZnO, InAlZnO, ZnTiO, ZnO, ZnAlO, and ZnCuO.
  • the main component of the semiconductor layer is any one of an oxide semiconductor containing indium (In) and oxygen (O), and an oxide semiconductor containing zinc (Zn) and oxygen (O) be able to.
  • the backing plate 13 b is made of metal, and the forming material of the backing plate 13 b is, for example, copper.
  • the target 13a described above is fixed to the backing plate 13b.
  • the entire cathode 13 may not be located in the vacuum chamber 11, and at least the surface to be sputtered of the target 13 a may be exposed in the vacuum chamber 11.
  • the sputtering apparatus 10 includes a target power supply 14 connected to a backing plate 13b.
  • a voltage is applied to the target 13a via the backing plate 13b.
  • the sputtering apparatus 10 further includes an exhaust unit 15 and a sputtering gas supply unit 16.
  • the exhaust unit 15 reduces the pressure of the film formation space divided by the vacuum chamber 11 to a predetermined pressure.
  • the exhaust unit 15 includes, for example, a pump and a valve.
  • the sputtering gas supply unit 16 supplies a sputtering gas used to generate a plasma for sputtering the target 13 a into the vacuum chamber 11.
  • the sputtering gas supply unit 16 is, for example, a mass flow controller that supplies sputtering gas at a predetermined flow rate, and is connected to a cylinder positioned outside the sputtering apparatus 10.
  • the sputtering gas supplied by the sputtering gas supply unit 16 may be, for example, a rare gas such as argon gas or an oxygen-containing gas such as oxygen gas.
  • the exhaust unit 15 decompresses the film formation space to a predetermined pressure.
  • the target power supply 14 applies a voltage to the target 13a via the backing plate 13b.
  • plasma is generated around the surface to be sputtered on the target 13a.
  • the sputtering target surface of the target 13a is sputtered by the positive ions in the plasma flying toward the target 13a.
  • a semiconductor layer mainly containing an oxide semiconductor is formed on the film formation surface of the film formation target S.
  • the plasma CVD apparatus 20 is equipped with the vacuum chamber 21 which divides the film-forming space for forming an insulator layer, The film-forming in which the semiconductor layer 31 was formed in the inside of the vacuum chamber 21
  • the support part 22 which supports object S is located.
  • the support part 22 is a stage which supports the laminated body of the semiconductor layer 31 and the film-forming object S, for example.
  • the diffusion portion 23 is positioned at a position facing the support portion 22.
  • the diffusion portion 23 has a function of diffusing the gas for forming the insulator layer into the vacuum chamber 21.
  • the diffusion unit 23 is, for example, a shower plate made of metal.
  • the diffusion unit 23 is also an example of an electrode provided in the plasma CVD apparatus 20.
  • the plasma CVD apparatus 20 includes an exhaust unit 24.
  • the exhaust unit 24 reduces the pressure in the film formation space divided by the vacuum chamber 21 to a predetermined pressure.
  • the exhaust unit 24 includes, for example, a pump and a valve, like the exhaust unit 15 of the sputtering apparatus 10.
  • the plasma CVD apparatus 20 further includes a film forming gas supply unit 25, an oxygen-containing gas supply unit 26, a heating unit 27, and a high frequency power supply 28.
  • the film forming gas supply unit 25 includes a thermostatic chamber 25a, a storage unit 25b, and a film forming gas supply unit 25c.
  • the constant temperature bath 25a divides a storage space for storing the storage unit 25b and the film forming gas supply unit 25c, and maintains the temperature of the storage space at a predetermined temperature.
  • the storage unit 25 b stores a liquid film forming material M. In the storage unit 25b, the film forming material M is in a state of gas-liquid equilibrium.
  • the film forming gas supply unit 25 c is a mass flow controller connected to the vacuum chamber 21 to supply the vaporized film forming material M into the vacuum chamber 21 at a predetermined flow rate.
  • the film forming gas supply unit 25 c supplies the gas of the film forming material M to the vacuum chamber 21 at a flow rate of, for example, 0.005 sccm / cm 2 or more and 0.1 sccm / cm 2 or less.
  • the film forming material M is, for example, tetraisocyanate silane (Si (NCO) 4 : TICS), and the plasma CVD apparatus 20 forms an insulator layer by a plasma CVD method using tetraisocyanate silane and oxygen. Since tetraisocyanate silane which is a raw material of the insulator layer does not contain hydrogen, the certainty that the concentration of hydrogen atoms in the insulator layer is 1 ⁇ 10 21 atoms / cm 3 or less is enhanced.
  • Si (NCO) 4 a material containing silicon (Si) and an isocyanate group (NCO) and containing no hydrogen can be used as the film forming material M.
  • any of Si (NCO) 3 Cl, Si (NCO) 2 Cl 2 and Si (NCO) Cl 3 can be used, for example.
  • a source gas which is a gas obtained by vaporizing the film forming material M is supplied to the vacuum chamber 21. That is, in forming the insulator layer, it is possible to use, as a source gas, a group consisting of Si (NCO) 4 , Si (NCO) 3 Cl, Si (NCO) 2 Cl 2 , and Si (NCO) Cl 3. Any one selected can be used.
  • the oxygen-containing gas supply unit 26 is connected to the vacuum chamber 21 via the heating unit 27.
  • the oxygen-containing gas supply unit 26 is, for example, a mass flow controller that supplies oxygen gas (O 2 ) to the vacuum tank 21 at a predetermined flow rate, and is connected to a cylinder located outside the plasma CVD apparatus 20.
  • the heating unit 27 heats the oxygen gas output from the oxygen-containing gas supply unit 26 to a predetermined temperature.
  • the heating unit 27 heats the oxygen gas to a temperature of, for example, 50 ° C. or more and 200 ° C. or less.
  • the oxygen-containing gas supply unit 26 may supply not only O 2 but also any one of O 3 , N 2 O, CO, and CO 2 as an oxygen-containing gas. That is, forming the insulator layer includes using any one selected from the group consisting of O 2 , O 3 , N 2 O, CO, and CO 2 as the oxygen-containing gas. obtain.
  • the oxygen-containing gas supplied from the oxygen-containing gas supply unit 26 may be supplied to the vacuum tank 21 in a state of being diluted with an inert gas.
  • an inert gas for example, N 2 , He, Ne, Ar, Kr, or Xe can be used.
  • High-frequency power source 28 for example, a high-frequency power having a frequency of 13.56MHz or 27.12 MHz, at 0.07 W / cm 2 or more 1.5 W / cm 2 or less in size, and supplies the spreading section 23.
  • the ratio of the power to the flow rate of the tetraisocyanate silane gas is preferably 17 W / sccm or more. This increases the reliability of forming an insulator layer having a hydrogen atom concentration of 1 ⁇ 10 21 atoms / cm 3 or less.
  • the exhaust unit 24 reduces the pressure in the vacuum chamber 21 to a predetermined pressure.
  • the film forming gas supply unit 25 c supplies tetraisocyanate silane gas to the vacuum chamber 21, and the oxygen-containing gas supply unit 26 supplies oxygen gas to the vacuum chamber 21, and then the high frequency power supply 28 supplies power to the diffusion unit 23. Supply.
  • a plasma is generated around the diffusion portion 23 from the above-described mixed gas.
  • an insulator layer mainly composed of silicon oxide is formed on the semiconductor layer 31.
  • forming the insulator layer comprises: supplying tetraisocyanate silane gas and oxygen gas to a deposition space for forming the insulator layer to produce a mixed gas; Supplying power to the diffusion unit 23, which is an example of an electrode located in the membrane space, to generate plasma from the mixed gas.
  • the active species generated from the tetraisocyanate silane gas is oxidized by the active species generated from the oxygen gas from the beginning of the plasma generation.
  • the thin film transistor 30 which is an example of the semiconductor device includes the semiconductor layer 31 and the insulator layer 32.
  • the semiconductor layer 31 includes the surface 31s, and in the semiconductor layer 31, an oxide semiconductor is a main component.
  • 90% by mass or more is an oxide semiconductor as in the case of the target 13a described above.
  • the insulator layer 32 is located on the surface 31s of the semiconductor layer 31.
  • silicon oxide is a main component and the concentration of hydrogen atoms is 1 ⁇ 10 21 / cm 3 or less.
  • the insulator layer 32 covers the surface 31 s of the semiconductor layer 31 and the portion of the gate insulator layer 35 not covered by the semiconductor layer 31.
  • the semiconductor layer 31 can include at least one semiconductor layer. That is, the semiconductor layer 31 may be composed of two or more semiconductor layers.
  • the main component of each semiconductor layer is preferably any one selected from the group consisting of InGaZnO, GaZnO, InZnO, InTiZnO, InAlZnO, ZnTiO, ZnO, ZnAlO, and ZnCuO.
  • the thin film transistor 30 includes the film formation target S described above, and the film formation target S includes the substrate 33, the gate electrode 34, and the gate insulator layer 35.
  • the gate electrode 34 is located on a part of the surface of the substrate 33, and the gate insulator layer 35 covers the entire gate electrode 34 and the surface of the substrate 22 not covered by the gate electrode 34.
  • the substrate 33 may be, for example, any of a resin substrate formed of various resins, and a glass substrate, and molybdenum or the like can be used as a material for forming the gate electrode 34, for example.
  • a silicon oxide layer or a stacked body of a silicon oxide layer and a silicon nitride layer can be used.
  • the semiconductor layer 31 is positioned to overlap the gate electrode 34 in the stacking direction of the layers constituting the thin film transistor 30 on the surface of the gate insulator layer 35.
  • the thin film transistor 30 further includes a source electrode 36 and a drain electrode 37, and the source electrode 36 and the drain electrode 37 are arranged at predetermined intervals in the arrangement direction (horizontal direction in FIG. 3) along the cross section of the thin film transistor 30. .
  • the source electrode 36 covers a part of the insulator layer 32, and the drain electrode 37 covers the other part of the insulator layer 32.
  • Each of the source electrode 36 and the drain electrode 37 is electrically connected to the semiconductor layer 31 through a contact hole formed in the insulator layer 32.
  • molybdenum or aluminum can be used as a forming material of the source electrode 36 and a forming material of the drain electrode 37.
  • the thin film transistor 30 further includes a protective film 38, which covers the source electrode 36 and the drain electrode 37 together with the portion of the insulator layer 32 exposed from both the source electrode 36 and the drain electrode 37.
  • a protective film 38 which covers the source electrode 36 and the drain electrode 37 together with the portion of the insulator layer 32 exposed from both the source electrode 36 and the drain electrode 37.
  • silicon oxide can be used as a material for forming the protective film 38.
  • Test examples will be described with reference to FIGS. 4 to 12.
  • Sample of laminate The configuration of the laminate 40 of the test example will be described with reference to FIG.
  • the laminate 40 in order to evaluate the influence of the hydrogen atoms contained in the insulator layer on the semiconductor layer, the laminate 40 described below with reference to FIG. 4 was used.
  • the laminate 40 includes a glass substrate 41, a semiconductor layer 42 located on a part of the surface of the glass substrate 41, and an insulator layer 43.
  • the insulator layer 43 is located on part of the surface of the semiconductor layer 42 and on the surface of the glass substrate 41 not covered by the semiconductor layer 42.
  • the insulator layer 43 includes a first portion 43A located on the surface of the semiconductor layer 42, and a second portion 43B sandwiching the first portion 43A in the arrangement direction (left and right direction in FIG. 4) along the cross section of the stacked body 40.
  • a third portion 43C is provided.
  • the first electrode layer 44A is located between the first portion 43A and the second portion 43B, and the first electrode layer 44A is a portion of the semiconductor layer 42, a portion of the first portion 43A, And a portion of the second portion 43B.
  • the second electrode layer 44B is located between the first portion 43A and the third portion 43C, and the second electrode layer 44B is a portion of the semiconductor layer 42, a portion of the first portion 43A, And a part of the third portion 43C.
  • the main component of the semiconductor layer 42 is IGZO, and the main component of the insulator layer 43 is SiO 2 .
  • the thickness of the semiconductor layer 42 is 50 nm, and the thickness of the insulator layer 43 is 100 nm.
  • the forming material of the first electrode layer 44A and the forming material of the second electrode layer 44B are Mo.
  • a semiconductor layer is formed on the surface of the glass substrate 41, and the semiconductor layer 42 is formed by etching the semiconductor layer through a mask.
  • an insulator layer is formed by plasma CVD over the entire surface of the semiconductor layer 42 and over the surface of the glass substrate 41 not covered by the semiconductor layer 42.
  • the insulator layer is etched through the mask to form the insulator layer 43 having the first portion 43A, the second portion 43B, and the third portion 43C.
  • a metal layer is formed to cover the semiconductor layer 42, the first portion 43A, the second portion 43B, and the third portion 43C of the insulator layer 43.
  • the metal layer is etched through the mask to form the first electrode layer 44A and the second electrode layer 44B.
  • the concentration of hydrogen atoms (pieces / cm 3 ), the concentration of carbon atoms (pieces / cm 3 ), and the concentration of oxygen atoms (pieces / cm 3 ) were each measured.
  • a secondary ion mass spectrometer (ADEPT1010, manufactured by ULVAC-PHI, Inc.) was used.
  • the concentration of hydrogen atoms in the insulator layer 43 decreases as the high frequency power when forming the insulator layer 43 increases.
  • the concentration of hydrogen atoms in the insulator layer 43 is 1 ⁇ 10 22 atoms / cm 3 when the high frequency power is 400 W, and 3 ⁇ 10 21 atoms / cm 3 when the high frequency power is 800 W. It was found to be 9 ⁇ 10 20 pieces / cm 3 when the power was 1000 W and 2 ⁇ 10 20 pieces / cm 3 when the high frequency power was 1600 W. It was also found that the concentration of hydrogen atoms was 9 ⁇ 10 19 atoms / cm 3 when the high frequency power was 3000 W, and 5 ⁇ 10 19 atoms / cm 3 when the high frequency power was 4000 W.
  • the ratio of the flow rate of the film forming gas to the high frequency power is 7 W / sccm when the high frequency power is 400 W, and the high frequency power is 800 W when the high frequency power is 800 W
  • the ratio of the flow rate of the deposition gas to the power is 15 W / sccm.
  • the ratio of the flow rate of the deposition gas to the high frequency power is 18 W / sccm when the high frequency power is 1000 W, and the ratio of the flow rate of the deposition gas to the high frequency power is 29 W / sccm when the high frequency power is 1600 W. is there.
  • the ratio of the flow rate of the deposition gas to the high frequency power is 55 W / sccm
  • the ratio of the flow rate of the deposition gas to the high frequency power is 72 W / sccm. That is, according to the measurement result of the concentration of hydrogen atoms, if the ratio of the flow rate of the film forming gas to the high frequency power is 17 W / sccm or more, the concentration of hydrogen atoms in the insulator layer is 1 ⁇ 10 21 atoms / cm 3 or less It is recognized that the certainty is increased.
  • the concentration of hydrogen atoms in the insulator layer is 4 ⁇ 10 21 atoms / cm 3
  • a silane gas When the insulator layer was formed using SiH 4 ), the concentration of hydrogen atoms in the insulator layer 43 was found to be 2 ⁇ 10 21 atoms / cm 3 .
  • the deposition conditions when using each of the TEOS gas and the SiH 4 gas were set as follows.
  • TEOS -Deposition gas tetraethoxysilane
  • Flow rate of deposition gas 100 sccm ⁇ Flow rate of 5000 sccm of oxygen gas ⁇ Pressure pressure of deposition space 175Pa ⁇ High frequency power 1600W ⁇ Area of electrode 2700 cm 2
  • SiH 4 -Deposition gas silane (SiH 4 ) ⁇ Flow rate of deposition gas 70 sccm -Flow rate of 3500 sccm of N 2 O gas ⁇ Pressure pressure of deposition space 200Pa ⁇ High frequency power 800W ⁇ Area of electrode 2700 cm 2
  • the concentration of carbon atoms in the insulator layer 43 is 3 ⁇ 10 19 / cm 3 when the high frequency power is 400 W, and 7 ⁇ 10 19 / cm 3 when the high frequency power is 800 W, and the high frequency power is When it was 1000 W, it was recognized to be 4 ⁇ 10 19 pieces / cm 3 .
  • the concentration of carbon atoms is 1 ⁇ 10 19 atoms / cm 3 when the high frequency power is 1600 W, 2 ⁇ 10 19 atoms / cm 3 when the high frequency power is 3000 W, and the high frequency power is 4000 W It was observed that it was 2 ⁇ 10 19 cells / cm 3 .
  • the concentration of nitrogen atoms in the insulator layer 43 increases as the high frequency power increases, and when the high frequency power is 1600 W or more It was found that the dependence of the nitrogen atom concentration on the magnitude of the high frequency power was small.
  • the concentration of nitrogen atoms in the insulator layer 43 is 4 ⁇ 10 19 atoms / cm 3 when the high frequency power is 400 W, and 2 ⁇ 10 20 atoms / cm 3 when the high frequency power is 800 W.
  • the power was 1000 W, it was found to be 2 ⁇ 10 20 cells / cm 3 .
  • the concentration of nitrogen atoms is 4 ⁇ 10 20 atoms / cm 3 when the high frequency power is 1600 W, 3 ⁇ 10 20 atoms / cm 3 when the high frequency power is 3000 W, and the high frequency power is 4000 W It was observed that it was 3 ⁇ 10 20 cells / cm 3 at a time.
  • the refractive index was measured in the insulator layer with which each laminated body is provided.
  • a spectroscopic ellipsometer (M-2000V, manufactured by J. A. Woolam) was used for the measurement of the refractive index.
  • the refractive index in the insulator layer 43 increases as the high frequency power when forming the insulator layer 43 increases.
  • the refractive index in the insulator layer 43 is 1.446 when the high frequency power is 400 W, 1.461 when the high frequency power is 800 W, and 1.464 when the high frequency power is 1000 W.
  • the refractive index was found to be 1.470 when the high frequency power was 1600 W, 1.473 when the high frequency power was 3000 W, and 1.479 when the high frequency power was 4000 W.
  • the film stress in the insulator layer 43 is -30 MPa when the high frequency power is 400 W, -140 MPa when the high frequency power is 800 W, and -196 MPa when the high frequency power is 1000 W.
  • the film stress was found to be -270 MPa when the high frequency power is 1600 W, -330 MPa when the high frequency power is 3000 W, and -398 MPa when the high frequency power is 4000 W.
  • Carrier concentration The carrier concentration was measured in the semiconductor layer included in each stack.
  • a Hall effect measuring device (HL55001U, manufactured by Nanometrics) was used to measure the carrier concentration.
  • the concentration of hydrogen atoms in the insulator layer 43 is higher than 1 ⁇ 10 21 atoms / cm 3 , the concentration of carriers in the semiconductor layer 42 is higher than 1 ⁇ 10 16 atoms / cm 3.
  • the concentration of hydrogen atoms in the insulator layer 43 is 1 ⁇ 10 21 atoms / cm 3 or less, it is recognized that the concentration of carriers in the semiconductor layer 42 is smaller than 1 ⁇ 10 13 atoms / cm 3. It was done.
  • the semiconductor when the concentration of hydrogen atoms in the insulator layer 43 is 1 ⁇ 10 21 atoms / cm 3 or less, the semiconductor has a concentration of hydrogen atoms that is higher than that of insulator layers greater than 1 ⁇ 10 21 atoms / cm 3. It was observed that the concentration of carriers in layer 42 was significantly reduced. Since the concentration of hydrogen atoms in the insulator layer 43 is 1 ⁇ 10 21 atoms / cm 3 or less, oxygen loss due to the reduction of the semiconductor layer 42 that is the lower layer of the insulator layer 43 is significantly suppressed. Is considered to have been obtained.
  • Example 1 A thin film transistor having the structure described above with reference to FIG. 3 and comprising a gate electrode, a gate insulator layer, a semiconductor layer, an insulator layer, a source electrode, a drain electrode, and a protective film. Formed.
  • the film forming conditions for the insulator layer were the same as those for TICS in the test example, and the film forming conditions for the semiconductor layer were the same as the test example.
  • the high frequency power at the time of forming the insulator layer was 1600 W.
  • the material for forming the gate electrode, the source electrode, and the drain electrode is molybdenum
  • the material for forming the gate insulator layer is silicon oxide
  • the material for forming the protective layer is silicon oxide.
  • Comparative Example 1 The thin film transistor of Comparative Example 1 was formed in the same manner as in Example 1 except that the film formation conditions for the insulator layer were the same as in Example 1 using SiH 4 in the test examples.
  • the transistor characteristics that is, the voltage (Vg) -current (Id) characteristics of each of the thin film transistor of Example 1 and the thin film transistor of Comparative Example 1 were measured using a semiconductor parameter analyzer (4155C, manufactured by Agilent Technologies). The measurement conditions of the transistor characteristics were set as follows.
  • the threshold voltage is 5.3 V
  • the on voltage is 0.66 V
  • the electron mobility is 10.2 V / cm 2 ⁇ cec. It was recognized that the subthreshold swing value was 0.31 V / decade.
  • the on voltage is a gate voltage when the drain current is 10 ⁇ 9 A / cm 2 .
  • the thin film transistor of Comparative Example 1 which includes an insulator layer having a concentration of hydrogen atoms larger than 1 ⁇ 10 21 / cm 3 does not operate normally, in other words, For example, the transistor characteristics were found to be unstable.
  • the following effects can be obtained. (1) Since the insulator layer 32 having a hydrogen atom concentration of 1 ⁇ 10 21 atoms / cm 3 or less is formed, the characteristics of the thin film transistor 30 can be stabilized.
  • the semiconductor device may include semiconductor elements other than the thin film transistor 30 as well as the thin film transistor 30 described above.
  • sputter gas supply part 20 plasma CVD apparatus 23: diffusion unit 25: deposition gas supply unit 25a: thermostatic chamber 25b: storage unit 25c: deposition gas supply unit 26: oxygen-containing gas supply unit 27: heating unit , 28: high frequency power source, 30: thin film transistor, 31, 42: semiconductor layer, 31s: surface, 32, 43: insulator layer, 33: substrate, 34: gate electrode, 35: gate insulator layer, 36: source electrode, 37: drain electrode, 38: protective film, 40: laminate, 41: glass substrate, 43A: first portion, 43B: second portion, 43C: third portion, 44A: first electrode layer 44B ... second electrode layer, M ... film-forming material, S ... film-forming target.

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